反应详情

100 mg (0.28 mmol) of 2-[3-(5-hydroxypyrimidin-2-yl)benzyl]-6-(1-methyl-1H-pyrazol-4-yl)-2H-pyridazin-3-one are dissolved in 6 ml of DMF, and 277 mg (0.83 mmol) of polymer-bound triphenylphosphine (3 mmol/g) and 33 mg (0.32 mmol) of 1,3-cyclopentanediol are added. The reaction mixture is shaken at room temperature for 15 min, and 196 mg (0.83 mmol) of di-tert-butyl azodicarboxylate are subsequently added. The reaction mix-ture was shaken at room temperature for 3 h, a further 277 mg (0.83 mmol) of polymer-bound triphenylphosphine (3 mmol/g) and 196 mg (0.83 mmol) of di-tert-butyl azodicarboxylate were added, and the mixture was shaken at room temperature for 18 h. The reaction mixture is filtered off through kieselguhr with suction and washed with acetonitrile. The filtrate is evaporated and purified by means of preparative HPLC.

1. additionThe reaction mix-ture
2. stirringwas shaken at room temperature for 3 h
3. stirringthe mixture was shaken at room temperature for 18 h
4. filtrationThe reaction mixture is filtered off through kieselguhr with suction
5. washwashed with acetonitrile
6. customThe filtrate is evaporated
7. custompurified by means of preparative HPLC